Water → HCID 59519496, compound

HRID 2102406Notes

Reaction equation

HRID 2102406 reaction equation
[Mn]([O-])(=O)(=O)=[O:2].[K+].[Cl:7][C:8]1[C:9]([CH3:18])=[N:10][C:11]2[N:12]([N:15]=[CH:16][CH:17]=2)[C:13]=1[F:14].[OH2:19]>>[Cl:7][C:8]1[C:9]([C:18]([OH:2])=[O:19])=[N:10][C:11]2[N:12]([N:15]=[CH:16][CH:17]=2)[C:13]=1[F:14]

Participants

4

Reactant 3

HCID 962WaterHCID 516875Potassium PermanganateHCID 69008047HCID 69008047, compound

Product 1

HCID 59519496HCID 59519496, compound

Conditions

Temperature
100 °C

Procedure

Potassium permanganate (2.00 equivalents) is added to 6-chloro-7-fluoro-5-methylpyrazolo[1,5-a]pyrimidine (1.00 equivalent) in water, and the mixture is heated at 100° C. After 3 hours, the reaction mixture is cooled to room temperature, and the precipitated oxides of manganese are filtered and washed with hot water. The filtrate is concentrated under reduced pressure, diluted with EtOAc, washed with 10% aqueous HCl solution, dried (MgSO4), and concentrated. The product may be triturated with an appropriate solvent such as diethyl ether or dichloromethane if further purification is necessary.

Workup

  1. temperaturethe reaction mixture is cooled to room temperature
  2. filtrationthe precipitated oxides of manganese are filtered
  3. washwashed with hot water
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. additiondiluted with EtOAc
  6. washwashed with 10% aqueous HCl solution
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated
  9. customThe product may be triturated with an appropriate solvent such as diethyl ether or dichloromethane if further purification

Sources & evidence

ORD record
ord-ea5325c710b648b8b03dd61f2c7a2549
Source dataset
uspto-grants-2009_08
Patent number
US07576072B2

Reaction notes

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